WO2019004589A1 - 질화 알루미늄 소결체 및 이를 포함하는 반도체 제조 장치용 부재 - Google Patents

질화 알루미늄 소결체 및 이를 포함하는 반도체 제조 장치용 부재 Download PDF

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WO2019004589A1
WO2019004589A1 PCT/KR2018/005369 KR2018005369W WO2019004589A1 WO 2019004589 A1 WO2019004589 A1 WO 2019004589A1 KR 2018005369 W KR2018005369 W KR 2018005369W WO 2019004589 A1 WO2019004589 A1 WO 2019004589A1
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Prior art keywords
aluminum nitride
sintered body
nitride sintered
titanium
weight
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PCT/KR2018/005369
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English (en)
French (fr)
Korean (ko)
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채재호
박효성
안덕원
강태희
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주식회사 미코
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Application filed by 주식회사 미코 filed Critical 주식회사 미코
Priority to CN201880035936.4A priority Critical patent/CN110770193A/zh
Priority to JP2019564032A priority patent/JP7181898B2/ja
Priority to CN202211132218.3A priority patent/CN115321987A/zh
Priority to US16/614,731 priority patent/US11508586B2/en
Publication of WO2019004589A1 publication Critical patent/WO2019004589A1/ko
Priority to US17/938,134 priority patent/US20230024625A1/en

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Definitions

  • the present invention relates to an aluminum nitride sintered body and a member for a semiconductor manufacturing apparatus including the same.
  • ceramic materials are used for electrostatic chucks for fixing wafers during a semiconductor manufacturing process, and heaters for semiconductor production in which wafers are fixed while heating them in a chemical vapor deposition (CVD) process.
  • CVD chemical vapor deposition
  • a ceramic material including aluminum nitride can be applied to a ceramic heater that heats a substrate as having a high thermal conductivity.
  • the ceramic heater includes a ceramic body, a reference potential layer for generating plasma in the body, and a heating element for generating heat.
  • ceramic materials including aluminum nitride require good electrical insulation and thermal conductivity.
  • the ceramic heater is required to function as an electrostatic chuck using an electrostatic force, a high volume resistance value at a high temperature is required.
  • the ceramic material constituting the ceramic heater needs to have a volume resistivity of 1.0 x 10 7 ? ⁇ Cm or more at a temperature of 500 ° C.
  • ceramic materials such as aluminum nitride have a volume resistivity that decreases with increasing temperature. Therefore, in the case of a ceramic heater using a ceramic material such as aluminum nitride, as the temperature increases, the volume resistance value of the ceramic body decreases, so that a leakage current may be generated between the reference potential layer and the heating layer. Furthermore, the ceramic heater can function as a sintering chuck, which may deteriorate the function.
  • a metal-based additive such as titanium, magnesium or silicon is added to the aluminum nitride constituting the ceramic body.
  • the additive deteriorates the thermal conductivity of the ceramic heater, thereby deteriorating the temperature uniformity of the ceramic heater.
  • the additive operates as a contaminant during operation of the semiconductor manufacturing apparatus.
  • an object of the present invention is to provide an aluminum nitride sintered body capable of maintaining the volume resistance at a high temperature while at the same time having an excellent thermal conductivity and suppressing the generation of impurities.
  • Another object of the present invention is to provide a member for a semiconductor manufacturing apparatus comprising the aluminum nitride sintered body.
  • the aluminum nitride sintered body according to one embodiment of the present invention comprises 1 to 5% by weight of yttrium oxide (Y 2 O 3 ), 10 to 100% by weight of titanium (Ti) And extra aluminum nitride (AlN).
  • Y 2 O 3 yttrium oxide
  • Ti titanium
  • AlN extra aluminum nitride
  • the weight ratio of the titanium to the yttrium oxide may be 0.0002 to 0.0031.
  • the aluminum nitride sintered body according to an embodiment of the present invention may have a volume resistance value in the range of 3.0 x 10 8 to 5.0 x 10 9 ? Cm at a temperature of 500 ° C and an electric field of 500 V / mm.
  • the aluminum nitride sintered body according to an embodiment of the present invention may have a thermal conductivity of 100 W / mK or more.
  • the aluminum nitride sintered body according to one embodiment of the present invention may be 30 ppb or less in the impurity inspection.
  • a member for a semiconductor manufacturing apparatus includes 1 to 5% by weight of yttrium oxide (Y 2 O 3 ), 10 to 100% by weight of titanium (Ti), and extra aluminum nitride (AlN)
  • Y 2 O 3 yttrium oxide
  • Ti titanium
  • AlN extra aluminum nitride
  • the weight ratio of the titanium to the yttrium oxide may be 0.0002 to 0.0031.
  • the aluminum nitride sintered body may have a volume resistance value in the range of 3.0 x 10 8 to 5.0 x 10 9 ? Cm m at a temperature of 500 ⁇ and an electric field of 500 V / mm.
  • the aluminum nitride sintered body may have a thermal conductivity of 100 W / mK or more.
  • the aluminum nitride sintered body may be 30 ppb or less in impurity inspection.
  • the aluminum nitride sintered body according to the present invention contains 1 to 5% by weight of yttrium oxide (Y 2 O 3 ), 10 to 100% by weight of titanium (Ti) and aluminum nitride (AlN). Accordingly, the aluminum nitride sintered body containing a small amount of titanium element and optimized yttrium oxide can maintain the volume resistance value at high temperature as well as secure an excellent thermal conductivity.
  • Y 2 O 3 yttrium oxide
  • Ti titanium
  • AlN aluminum nitride
  • the semiconductor manufacturing member using the aluminum nitride sintered body is used in a semiconductor manufacturing process, the content of titanium serving as a contamination source is limited, so that defective incidence in the manufacturing process can be reduced.
  • FIG. 1 is a cross-sectional view illustrating a member for a semiconductor manufacturing apparatus according to an embodiment of the present invention.
  • first, second, etc. may be used to describe various components, but the components should not be limited by the terms. The terms are used only for the purpose of distinguishing one component from another.
  • first component may be referred to as a second component, and similarly, the second component may also be referred to as a first component.
  • the aluminum nitride sintered body according to the present invention includes yttrium oxide, titanium and aluminum nitride.
  • the aluminum nitride (AlN) contained in the sintered body of the present invention has high thermal conductivity and high electrical insulating properties. Therefore, the aluminum nitride (AlN) serves to make the aluminum nitride sintered body have properties of high thermal conductivity and high insulation.
  • the aluminum nitride sintered body containing aluminum nitride can be applied to an electrostatic chuck type heating plate which simultaneously heats and fixes the wafer.
  • a high purity (99% or more) reduced aluminum nitride powder can be used as the raw material powder of aluminum nitride.
  • the aluminum nitride sintered body of the present invention includes yttrium oxide (Y 2 O 3 ).
  • the weight percentage of yttrium oxide is a method of confirming the amount of the element detected when an aluminum nitride sintered body is measured using a scanning electron microscope or an energy dispersive X-ray spectroscope mounted on a transmission electron microscope .
  • the yttrium oxide weight% can be calculated by converting the content of yttrium detected into an oxide.
  • the yttrium oxide causes the aluminum nitride sintered body to have a thermal conductivity of a predetermined value or more. That is, yttrium oxide functions to compensate for the decrease in thermal conductivity due to the addition of titanium.
  • the yttria serves to assist sintering between the components in the process of manufacturing the aluminum nitride sintered body.
  • yttrium when yttrium is added in the form of an oxide, it may exist as an aluminate compound by reacting with oxygen and aluminum contained in the aluminum nitride sintered powder.
  • the aluminate compound has a relatively low firing temperature.
  • the yttria facilitates sintering by reacting with other elements for producing a sintered body, thereby lowering the sintering temperature during sintering. Therefore, the aluminum nitride sintered body of the present invention includes yttrium oxide, thereby facilitating the sintering process and enhancing the compactness of the sintered body.
  • the yttrium oxide may have a composition ratio ranging from 1 to 5% by weight based on the weight of the entire aluminum nitride sintered body.
  • the mechanical strength of the aluminum nitride sintered body may be lowered. There is no significant contribution to the volume resistance of the aluminum nitride sintered body even if the yttria exceeds the proper amount. Further, the appearance of the aluminum nitride sintered body, such as brightness or saturation, may be deteriorated.
  • the aluminum nitride sintered body of the present invention includes titanium (Ti).
  • the titanium (Ti) may have a composition ratio of 10 to 100 ppm by weight based on the weight of the entire aluminum nitride sintered body.
  • the titanium serves to increase the volume resistance value of the aluminum nitride sintered body. That is, when the sintered body is produced by adding yttrium oxide and titanium to the aluminum nitride together, the sintered body has a volume resistivity of 3.0 ⁇ 10 8 to 5.0 ⁇ 10 9 ⁇ ⁇ cm at a temperature of 500 ° C. and an electric field of 500 V / Lt; / RTI > Therefore, when the aluminum nitride sintered body is applied to the ceramic heater and the temperature of the ceramic heater is increased, the ceramic heater maintains a certain volume resistance value, so that the leakage current that can be generated in the ceramic heater can be suppressed.
  • the content of titanium added to the sintered body exceeds 100 wt ppm (0.01 wt%), the color of the aluminum nitride may change, and the physical properties of the aluminum nitride sintered body such as hardness and thermal conductivity may be deteriorated.
  • the increase in the volume resistivity of the aluminum nitride sintered body effect due to titanium insufficient to without the volume resistivity of the aluminum nitride sintered body increases further, 3 ⁇ 10 9 ⁇ ⁇ cm to 4.0 ⁇ maintain a volume resistivity of 10 9 ⁇ ⁇ cm range Only.
  • the aluminum nitride sintered body may not be independently existed in the state of titanium nitride (TiN) at high temperature, but may be connected to each other, and the volume resistance value may be drastically reduced.
  • the product is immersed in a liquid such as isopropyl alcohol (IPA) and the surface of the product is rubbed for a predetermined time. Thereafter, the number of impurities existing in the liquid is counted.
  • IPA isopropyl alcohol
  • the titanium (Ti) element corresponds to an impurity during a semiconductor process, and can act as a process contamination source in a semiconductor process.
  • the semiconductor manufacturing apparatus may cause contamination due to impurities Can be serious.
  • the titanium (Ti) may have a composition ratio ranging from 10 to 100 ppm by weight based on the weight of the entire aluminum nitride sintered body.
  • Aluminum nitride sintered body powder prepared by mixing yttria (Y 2 O 3 ) powder, titanium oxide (TiO 2 ) powder and extra aluminum nitride (AlN) powder based on the total weight of the aluminum nitride sintered body is prepared. At this time, as the aluminum nitride powder, a high purity reduced aluminum nitride powder can be prepared. At this time, the composition ratio of the yttrium oxide (Y 2 O 3 ) powder, the titanium oxide (TiO 2 ) powder and the extra aluminum nitride (AlN) can be adjusted.
  • the aluminum nitride sintered body powder is dry-mixed or wet-mixed.
  • the mixing is carried out by a wet mixing method.
  • a wet mixing method for example, anhydrous ethanol, isopropyl alcohol and the like can be used as the solvent.
  • the slurry is extracted and dried by a spray drying method or the like to obtain a mixed powder.
  • the mixture is dried in a drier at about 60 to about 100 < 0 > C.
  • the aluminum nitride sintered body powder is sieved using a sieve, and then the aluminum nitride sintered body powder is sintered in a suitable shaped body. After sintering, the sintered aluminum nitride powder is sintered. According to one embodiment of the present invention, sintering is performed by baking at a temperature of about 1,700 to about 2,000 DEG C for at least about 30 minutes. For example, the aluminum nitride sintered body powder is charged into a graphite mold and fired in a high-temperature sintering furnace at a sintering temperature of about 1,850 ° C under a nitrogen atmosphere for about 3 hours, followed by cooling to form a sintered aluminum nitride body.
  • the weight% of yttrium oxide means a value calculated by adding the weight of the yttrium oxide powder added to the weight of the hydrate, chloride, and other types of precursors including yttrium to the yttrium oxide weight.
  • a high purity reduced aluminum nitride powder was prepared as the aluminum nitride powder.
  • the purity of the reduced aluminum nitride powder excluding oxygen was 99.9% or more, and the average particle diameter was about 1.3 ⁇ ⁇ .
  • the yttria powder having a purity of 99.9% or more and an average particle diameter of about 0.8 ⁇ ⁇ was used, and the titanium oxide powder having a purity of 99.9% or more and an average particle diameter of about 1.0 ⁇ ⁇ was used.
  • the weight% of yttrium oxide and the weight (ppm) of titanium were measured in the following manner.
  • the sintered aluminum nitride sintered body is measured by using an energy dispersive X-ray spectroscope equipped with a scanning electron microscope or a transmission electron microscope to confirm the amount of the element detected.
  • the wt% yttria was calculated by converting the content of yttrium detected to oxide. Also, the amount of titanium element was measured by ICP MS analysis.
  • Examples 2 to 7 and Comparative Examples 1 to 9 aluminum nitride sintered bodies were produced in the same manner as in Example 1, and the composition ratios of aluminum nitride, yttrium oxide and titanium were adjusted as shown in the following table.
  • Example 1 99 One 10 0.0010 0.0010 Example 2 99 One 31 0.0031 0.0031 Example 3 97 3 17 0.0017 0.0006 Example 4 97 3 83 0.0083 0.0028 Example 5 95 5 21 0.0021 0.0004 Example 6 95 5 100 0.0100 0.0020 Example 7 90 10 23 0.0023 0.0002 Comparative Example 1 95 5 1000 0.1000 0.0026 Comparative Example 2 95 5 130 0.0130 0.0020 Comparative Example 3 95 5 0 0 0 Comparative Example 4 100 0 0 0 - Comparative Example 5 100 0 6 0.0006 - Comparative Example 6 100 0 19 0.0019 - Comparative Example 7 100 0 35 0.0035 - Comparative Example 8 95 5 9 0.0009 0.0002 Comparative Example 9 90 10 9 0.0009 0.0002 Comparative Example 9 90 10 9 0.0009
  • Volumetric resistance Samples of aluminum nitride sintered bodies produced according to Examples 1 to 7 and Comparative Examples 1 to 9 were prepared so as to have dimensions of 50 mm x 50 mm x 1 mm thick, and the electrode shapes were measured with a main electrode diameter of 26 mm and a protective electrode diameter of 38 mm The applied voltage was set to 500 V / mm based on the applied electric field, and the volume resistance value obtained after maintaining the voltage application time for 60 seconds was recorded.
  • Impurity test method The sintered body specimen is immersed in a liquid such as IPA and the surface of the specimen is rubbed for 10 minutes. Thereafter, the number of impurities existing in the liquid is counted.
  • Thermal Conductivity Measurement Method The surface of the specimen of the aluminum nitride sintered body was blackened, and then the diffusion coefficient was calculated by the laser flash method. Using the diffusion coefficient, the thermal conductivity was derived from equation (1).
  • the aluminum nitride sintered bodies according to Examples 1 to 7 of the present invention each have a volume resistance value at a high temperature (500 ° C) of 3.0 x 10 8 to 5.0 x 10 9 ⁇ cm, and less than 50 ppb And a thermal conductivity of 125 W / mK or more is suitable for the heater member.
  • a member for a semiconductor manufacturing apparatus includes a heating plate 110, a conductive member 120, and a power supply unit 140.
  • the heating plate 110 supports the substrate 10 using an electrostatic force.
  • the heating plate 110 is provided to heat the substrate.
  • the heating plate 110 has a disk shape.
  • the supporting member serves to support the heating plate 110 so as not to be tilted.
  • the support member may also be made of a stainless steel alloy, an aluminum alloy, or a copper alloy.
  • the heating plate 110 is composed of an aluminum nitride sintered body.
  • the aluminum nitride sintered body includes yttrium oxide, titanium and aluminum nitride.
  • the aluminum nitride sintered body of the present invention including aluminum nitride may be used as a heating plate 110 such as a heater for fixing and heating a wafer in a semiconductor manufacturing process.
  • the titanium serves to increase the volume resistance value of the aluminum nitride sintered body.
  • a dielectric layer (not shown) may be further formed on the upper surface of the heating plate 110.
  • the conductive member 120 is buried in the heating plate 110.
  • the conductive member 120 functions as an electrostatic field generating electrode, a high frequency generating electrode, a heating element, or the like.
  • the conductive member 120 is made of metal.
  • the conductive member 120 may be formed of a conductive material such as tungsten (W), titanium (Ti), rhodium (Rh), niobium (Nb), iridium (Ir), rhenium (Re), tantalum (Ta), molybdenum And combinations of these.
  • connection cable 125 electrically connected to the conductive member 120 is provided under the conductive member 120.
  • the connection cable 125 is made of a metal having a small contact resistance with the conductive member 120 and having excellent electrical conductivity.
  • the connection cable 125 is connected to a power supply 140 for supplying power to the conductive member 120.
  • the power supplied from the power supply unit 140 to the conductive member 120 can be variously selected. For example, a DC chucking voltage may be applied to generate an electrostatic field from the power supply 140 to the conductive member 120 over the plate 110, and a high frequency bias power may be applied to generate a plasma And a general AC voltage may be supplied to generate heat from the conductive member 120.
  • the aluminum nitride sintered body according to the embodiments of the present invention can be applied to an electrostatic chuck for fixing a wafer and a heater for semiconductor manufacturing in which a wafer is fixed while being heated in a chemical vapor deposition (CVD) process or the like.
  • CVD chemical vapor deposition

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PCT/KR2018/005369 2017-06-30 2018-05-10 질화 알루미늄 소결체 및 이를 포함하는 반도체 제조 장치용 부재 WO2019004589A1 (ko)

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CN201880035936.4A CN110770193A (zh) 2017-06-30 2018-05-10 氮化铝烧结体及包括其的半导体制造装置用构件
JP2019564032A JP7181898B2 (ja) 2017-06-30 2018-05-10 窒化アルミニウム焼結体およびこれを含む半導体製造装置用部材
CN202211132218.3A CN115321987A (zh) 2017-06-30 2018-05-10 氮化铝烧结体及包括其的半导体制造装置用构件
US16/614,731 US11508586B2 (en) 2017-06-30 2018-05-10 Aluminum nitride sintered body and member for semiconductor manufacuting apparatus comprising same
US17/938,134 US20230024625A1 (en) 2017-06-30 2022-10-05 Aluminum nitride sintered body and member for semiconductor manufacuting apparatus comprising same

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